CN102528075B - Method for preparing ultrafine silver powder by directly performing thermal decomposition on silver nitrate - Google Patents
Method for preparing ultrafine silver powder by directly performing thermal decomposition on silver nitrate Download PDFInfo
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- CN102528075B CN102528075B CN 201210069052 CN201210069052A CN102528075B CN 102528075 B CN102528075 B CN 102528075B CN 201210069052 CN201210069052 CN 201210069052 CN 201210069052 A CN201210069052 A CN 201210069052A CN 102528075 B CN102528075 B CN 102528075B
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Abstract
The invention discloses a method for preparing ultrafine silver powder by directly performing thermal decomposition on silver nitrate. The method comprises the following steps of: putting a crucible with a silver nitrate solid into a tubular furnace, heating to temperature of between 400 and 550 DEG C at heating speed of between 5 and 50 DEG C/min, and introducing air with the relative humidity of between 80 and 100 percent, wherein the air flow is of between 200 and 800 ml/min; calcining for 2 to 8 hours, stopping heating and introducing the air; and cooling to room temperature, collecting solid products in the crucible, and thus obtaining the ultrafine silver powder with the average particle size of between 0.5 and 2 mu m. According to the method, reducing agents and aids are not required. The process is simple, and is low in cost; and the obtained silver powder is similarly spherical particles, has high purity, high crystallinity and relatively high compaction density, and is suitable for conductive slurry industries.
Description
Technical field
The present invention relates to a kind of preparation method of super fine silver powder, be specifically related to decompose with the silver nitrate direct heat method for preparing super fine silver powder, belong to the metal powder preparation technical field.
Background technology
Silver powder, owing to having splendid electrical and thermal conductivity and anti-oxidant zinc is strong, therefore is widely used in electronics industry.Silver powder is as the basic material of thick-film electronic slurry, its technology of preparing is study hotspot always, the particularly rise of solar energy industry, make each association area sharply increase the silver powder consumption figure, but the performance to silver powder is also had higher requirement, as spherical or class spherical morphology, single dispersion, high-tap density etc.
The preparation technology of silver powder is more, mainly contains atomization, spray pyrolysis, electrolysis, liquid phase reduction etc.As denomination of invention is " a kind of manufacture method of hydraulic atomized silver powder " (Chinese Patent Application No. is 96105437.9), provide a kind of atomization to prepare the method for silver powder: to adopt water or gas as atomizing medium, fine silver liquid stream to impact fusion after its pressurization, make it be atomized into silver powder.Atomization gained morphologies be irregular spherical, granularity is thicker, is generally about 40um, therefore is difficult to meet the requirement of electrocondution slurry.Denomination of invention is: " a kind of preparation method of ball shape silver powder " (Chinese Patent Application No. is 201110076231.7), provide a kind of spray pyrolysis to prepare the method for silver powder: by after the soluble silver salt solution atomization, carry out pyrolysis under high temperature controlled atmosphere condition, can obtain the silver powder product.This technique is comparatively simple, the gained morphologies is regular spherical but product granularity is thick and equipment manufacturing cost is comparatively expensive, and the industrialization difficulty is larger.It is anode that electrolysis be take thick silver or fine silver plate usually, and the titanium plate is negative electrode, HNO
3+ AgNO
3system is electrolyte, controls certain electrolysis system, can on negative electrode, obtain the silver powder product.Electrolysis silver powder granularity is 10-20um, and pattern is dendroid, mainly is widely used in the production of electrical alloy.The liquid phase reduction process is simple, be easy to control powder morphology and granularity, and research and application are comparatively extensive.At liquid phase reduction, prepare in silver powder, general by changing argentiferous presoma, reducing agent and dispersant, and regulate the reaction conditions such as concentration, temperature, stirring stream shape and intensity, realize the control to powder morphology and granularity.Its essence is the degree of supersaturation of the hierarchy of control and the active force between silver-colored particulate, regulates forming core, growth and the reunion behavior of silver powder particles.The silver powder formed under high degree of supersaturation, reunion is serious, monodispersity is poor, degree of crystallinity is low, tap density is little, is difficult to meet the requirement for preparing the crystal silicon solar energy battery positive silver paste.Usually the pyrolysis temperature of the direct pyrolysis of silver nitrate is higher, causes the silver powder easy-sintering, forms bulk or sheet, thereby can not get silver powder.
Summary of the invention
The object of the invention is to overcome the deficiency of prior art and a kind of method prepare super fine silver powder of decomposing by direct heat is provided.
A kind of method for preparing super fine silver powder of decomposing by direct heat of the present invention is to adopt following proposal to realize:
The crucible that fills the silver nitrate solid is put into to tube furnace, firing rate with 5-50 ℃/min is heated to 400-550 ℃, and pass into the air that relative humidity is 80-100%, air mass flow is 200-800ml/min, after calcining 2-8h, stop heating and ventilation, be cooled to room temperature, collect solid product in crucible, obtain super fine silver powder; Waste gas decomposition after absorbing, by-product nitric acid.
Super fine silver powder exterior appearance prepared by the inventive method is spherical particle, and average grain diameter is 0.5-2um, and product purity is high, and crystallization is high.
The present invention, owing to adopting above-mentioned process, in the situation that there is steam to exist, can effectively avoids the sintering of silver nitrate thermal decomposition gained silver powder, thereby obtain the super fine silver powder that average grain diameter is 0.5-2um.
Compared with prior art, the advantage of the inventive method is:
(1) technique is simple, flow process is short, without the operations such as liquid-solid separation, drying in the liquid phase production method.
(2) simple without especial equipment requirements, technological equipment, invest little, cost is low.
(3) discharge environmental friendliness in production process without waste water,waste gas and industrial residue;
(4) in production process, except can obtaining the silver powder product, also can obtain salpeter solution, the comprehensive utilization of resources rate is high.
(5) superior product quality is embodied as: thermal decomposition gained silver powder degree of crystallinity is high, tap density is large; In addition, because flow process is short, avoided the introducing of impurity in the production process, thereby purity is higher.
The accompanying drawing explanation
The silver powder X diffraction analysis result that accompanying drawing 1 is the embodiment of the present invention 1 preparation.
The stereoscan photograph (10000X) of the silver powder that accompanying drawing 2 is the embodiment of the present invention 1 preparation.
The stereoscan photograph (10000X) of the silver powder that accompanying drawing 3 is the embodiment of the present invention 2 preparations.
Can find out from accompanying drawing 1, outside the characteristic peak of desilver, there is no other dephasigns, and the characteristic peak of sample is narrow and sharp-pointed, shows that gained silver powder degree of crystallinity is higher.
From accompanying drawing 2, the morphologies of embodiment 1 preparation is spherical particle, and particle mean size is the 1.5um left and right.
From accompanying drawing 3, the morphologies of embodiment 2 preparations is spherical particle, and particle mean size is the 0.8um left and right.
The specific embodiment
Embodiment 1:
The crucible that fills 40g silver nitrate solid is put into to tube furnace, firing rate with 5 ℃/min is heated to 440 ℃, and pass into the air that relative humidity is 80-85%, air mass flow is 400-500ml/min, after calcining 6h, stop heating and ventilation, be cooled to room temperature, collect solid product in crucible, obtain the super fine silver powder product.The X diffraction analysis collection of illustrative plates of gained silver powder as shown in Figure 1, can be found out from scheming, and outside the characteristic peak of desilver, there is no other dephasigns, and the characteristic peak of sample is narrow and sharp-pointed, shows that gained silver powder degree of crystallinity is higher.As shown in Figure 2, as seen from the figure, the gained morphologies is spherical particle to the stereoscan photograph of gained silver powder, and particle mean size is the 1.5um left and right.
Embodiment 2:
The crucible that fills 40g silver nitrate solid is put into to tube furnace, firing rate with 20 ℃/min is heated to 520 ℃, and passes into the air that relative humidity is 85-90%, and air mass flow is 600-800ml/min, after calcining 4h, stop heating and ventilation, be cooled to room temperature, collect solid product in crucible, obtain stereoscan photograph that the super fine silver powder product obtains silver powder as shown in Figure 3, as seen from the figure, the gained morphologies is spherical particle, and particle mean size is the 0.8um left and right.
Embodiment 3:
The crucible that fills 40g silver nitrate solid is put into to tube furnace, firing rate with 35 ℃/min is heated to 400 ℃, and pass into the air that relative humidity is 80-85%, air mass flow is 200-300ml/min, after calcining 8h, stop heating and ventilation, be cooled to room temperature, collect solid product in crucible, obtain the super fine silver powder product.The gained morphologies is spherical particle, and the silver powder granularity is 1.2um.
Embodiment 4:
The crucible that fills 40g silver nitrate solid is put into to tube furnace, firing rate with 50 ℃/min is heated to 550 ℃, and passing into the air that relative humidity is 95-95%, air mass flow is 350-450ml/min, after calcining 2h, stop heating and ventilation, be cooled to room temperature, collect solid product in crucible, obtain the super fine silver powder product, the gained morphologies is spherical particle, and the silver powder granularity is 1um.
Claims (3)
1. one kind is decomposed the method for preparing super fine silver powder with the silver nitrate direct heat, be characterised in that: the crucible that will fill the silver nitrate solid is put into tube furnace, with 5 ?the firing rate of 50 ℃/min be heated to 400-440 ℃, and pass into the air that relative humidity is 80-100%, air mass flow is 200-800ml/min, after calcining 2-8h, stops heating and ventilation, be cooled to room temperature and can in crucible, collect solid product, obtain super fine silver powder.
2. a kind of method prepare super fine silver powder of decomposing with the silver nitrate direct heat according to claim 1 is characterised in that: waste gas decomposition after absorbing, by-product nitric acid.
3. a kind of method prepare super fine silver powder of decomposing with the silver nitrate direct heat according to claim 1, be characterised in that: described super fine silver powder pattern is spherical particle, granularity 0.5 ?2um.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201210069052 CN102528075B (en) | 2012-03-15 | 2012-03-15 | Method for preparing ultrafine silver powder by directly performing thermal decomposition on silver nitrate |
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| CN 201210069052 CN102528075B (en) | 2012-03-15 | 2012-03-15 | Method for preparing ultrafine silver powder by directly performing thermal decomposition on silver nitrate |
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| CN102528075A CN102528075A (en) | 2012-07-04 |
| CN102528075B true CN102528075B (en) | 2013-12-18 |
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| JP6189740B2 (en) * | 2013-05-24 | 2017-08-30 | 田中貴金属工業株式会社 | Method for producing silver particles |
| CN104057096B (en) * | 2014-06-23 | 2016-01-20 | 北京科技大学 | In biological adsorption solution, valuable metal ions prepares the method for superfine powdery material |
| CN109702222B (en) * | 2018-03-30 | 2022-06-10 | 中南大学 | Preparation method of silver zinc oxide or silver copper oxide composite powder and system for implementing preparation method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1323671A (en) * | 2000-05-02 | 2001-11-28 | 昭荣化学工业株式会社 | Method for prepn. of metal powder |
| CN1494966A (en) * | 2002-09-10 | 2004-05-12 | ���ٻ�ѧ��ҵ��ʽ���� | Method for mfg. metal powder |
| CN102114546A (en) * | 2011-03-29 | 2011-07-06 | 兰州金川新材料科技股份有限公司 | Method for preparing spherical silver powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH05311212A (en) * | 1992-05-01 | 1993-11-22 | Tanaka Kikinzoku Kogyo Kk | Production of fine powder of ag-pd alloy powder |
| JP2002294312A (en) * | 2001-03-29 | 2002-10-09 | Toda Kogyo Corp | Method for manufacturing metal particle powder |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1323671A (en) * | 2000-05-02 | 2001-11-28 | 昭荣化学工业株式会社 | Method for prepn. of metal powder |
| CN1494966A (en) * | 2002-09-10 | 2004-05-12 | ���ٻ�ѧ��ҵ��ʽ���� | Method for mfg. metal powder |
| CN102114546A (en) * | 2011-03-29 | 2011-07-06 | 兰州金川新材料科技股份有限公司 | Method for preparing spherical silver powder |
Non-Patent Citations (2)
| Title |
|---|
| SP法制备球形的金属银超细粉体;金宗莲等;《上海金属》;20010331;第23卷(第2期);第37-40页 * |
| 金宗莲等.SP法制备球形的金属银超细粉体.《上海金属》.2001,第23卷(第2期),第37-40页. |
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